CN110265644B - Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure - Google Patents

Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure Download PDF

Info

Publication number
CN110265644B
CN110265644B CN201910548720.4A CN201910548720A CN110265644B CN 110265644 B CN110265644 B CN 110265644B CN 201910548720 A CN201910548720 A CN 201910548720A CN 110265644 B CN110265644 B CN 110265644B
Authority
CN
China
Prior art keywords
carbon cloth
polyacrylic acid
ion battery
porous structure
mesh
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910548720.4A
Other languages
Chinese (zh)
Other versions
CN110265644A (en
Inventor
费杰
王娜
黄剑锋
曹丽云
许占位
李嘉胤
郑欣慧
李盟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201910548720.4A priority Critical patent/CN110265644B/en
Publication of CN110265644A publication Critical patent/CN110265644A/en
Application granted granted Critical
Publication of CN110265644B publication Critical patent/CN110265644B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/366Composites as layered products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621Binders
    • H01M4/622Binders being polymers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a preparation method of a mesh porous structure antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material, which comprises the following steps of 1: soaking the carbon cloth in acetone, cleaning and drying, soaking the dried carbon cloth in polyacrylic acid aqueous solution, coating, cleaning and drying again; step 2: adding antimony trichloride into absolute ethyl alcohol to form an antimony trichloride solution, and adding a sodium hydroxide aqueous solution into the antimony trichloride solution to adjust the pH value of the antimony trichloride solution to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution; and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a reaction kettle for hydrothermal reaction, cooling to room temperature, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with the mesh-shaped porous structure. The flexible electrode is simple to operate and good in repeatability, combines the characteristics of good mechanical property of carbon cloth and high specific capacity of antimony pentoxide, and improves the electrochemical cycle performance of the cathode material of the sodium-ion battery.

Description

Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure
Technical Field
The invention belongs to the technical field of flexible energy storage materials, and particularly relates to a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode material with a mesh-shaped porous structure.
Background
With the development of flexible and bendable electronic devices, the development of flexible electrode materials with high specific capacity has become an important direction for research in the field of energy storage. At present, the main flexible electrode material usually adopts carbon materials with good conductivity, such as graphene, carbon nanotubes, carbon cloth and the like. In which carbon cloth is widely used as a flexible electrode due to its good mechanical strength, electrical conductivity and flexibilityA material substrate. In recent years, many researchers have used flexible electrode materials by growing active materials such as metal oxides on carbon cloths. LongH et al directly grow NiO nanoplates on a carbon cloth substrate by a solution method and an annealing treatment method, and use the NiO nanoplates as a flexible negative electrode of a lithium ion battery (Growth of high-purity mesoporous NiO nanoplates on carbon cathodes as binders-free anodes for high-performance flexible lithium-ion batteries [ J]Scientific reports,2014,4: 7413). ZhangY et al prepared a flexible MoSe by solvothermal method2/CF composite material (MoSe)2nanosheets grown on carbon cloth with superiorelectrochemical performance as flexible electrode for sodium ion batteries[J]RSC Advances,2015,6(2): 1440-1444). Synthesis of Na by SangHJ et al by Sol-gel method2FeP2O7The composite material with the porous carbon cloth as the flexible negative electrode material of the sodium-ion battery has good long-term circulation capability (the sodium-ion battery with the porous materials with the porous rate capability and the porous carbon cloth with the good long-term circulation capability2FeP2O7nanoparticles on porous carbon cloth[J]Journal of materials chemistry A,2017,5(11): 5502-. RenWN et al atomic layer deposition of TiO2Layer to decorate three-dimensional flower-shaped MoS2Nano-sheet carbon cloth composite (ALD TiO)2coated flower-like MoS2nanosheets on carboncloth as sodium ion battery anode with enhanced cycling stability andratecapability[J].ACS Applied Materials&Interfaces,2016,9(1): 487-. However, the above method does not involve the problems of bonding between the carbon cloth and the supported active material and uniformity of growth morphology.
Research on the negative active material of the sodium-ion battery mainly focuses on carbon materials, alloy materials and compound materials. Each of the materials has merits, and among them, metal compound materials have been widely studied due to their large specific capacities. China is a country with large antimony reserves, antimony is in the fifth main group of the periodic table and has two valence states, namely trivalent valence and pentavalent valence, and the corresponding oxide is Sb2O3And Sb2O5. Wherein Sb2O3Has higher theoretical capacity (1102 mAhg)-1) Is in large quantityStudy of Sb2O5Reports on battery materials have not been made.
Disclosure of Invention
The invention aims to provide a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a reticular porous structure, which is simple to operate, low in cost, green, environment-friendly and good in binding force.
In order to realize the purpose, the invention is realized by the following technical scheme:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: soaking the carbon cloth in acetone to remove surface impurities, cleaning and drying, soaking the dried carbon cloth in polyacrylic acid aqueous solution for coating treatment, cleaning and drying;
step 2: adding 0.3-1.14 g of antimony trichloride into 20-60 mL of absolute ethanol, stirring to form an antimony trichloride solution, adding a sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value of the aqueous solution to 8-12 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution;
and step 3: and (3) transferring the carbon cloth and the mixed solution obtained in the step (2) to a reaction kettle for hydrothermal reaction at 120-180 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-shaped porous structure.
Further, the carbon cloth in the step 1 is soaked in acetone for 24-72 hours.
Further, in the step 1, the mass concentration of the polyacrylic acid aqueous solution is 1-8 mg/mL, and the time for immersing the dried carbon cloth into the polyacrylic acid aqueous solution for coating treatment is 1-12 h.
Further, polyacrylic acid has an average molecular weight of 1250000.
Further, the cleaning in step 1 and step 3 is repeated by using deionized water and ethanol respectively.
Further, the carbon cloth coated in the step 2 is placed into the mixed liquid to be soaked and stirred for 20-40 min.
Furthermore, the mass concentration of the sodium hydroxide aqueous solution in the step 2 is 0.03-0.12 g/mL.
Further, in the step 3, the reaction kettle is a polytetrafluoroethylene kettle, the carbon cloth and the mixed solution are transferred to the polytetrafluoroethylene kettle and placed in a homogeneous phase reactor for hydrothermal reaction for 4-48 h.
Further, the carbon cloth is hydrophilic carbon cloth and has a specification of 4cm × 2 cm..
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a preparation method of a mesh porous structure antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material, which comprises the steps of soaking cleaned carbon cloth in a polyacrylic acid aqueous solution for coating treatment; then taking out the carbon cloth, cleaning and drying; then putting the dried carbon cloth into an antimony trichloride ethanol solution, taking a sodium hydroxide aqueous solution as a precipitator, and then carrying out hydrothermal reaction to prepare a mesh porous structure antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material; the carbon cloth substrate is coated with a layer of polyacrylic acid high molecular adhesive, which can form better combination with the carbon cloth substrate, and polyacrylic acid molecules contain a large amount of carboxyl groups which are uniformly distributed and can be uniformly mixed with Sb2O5Firm chemical bonding is formed, and the problems that the carbon cloth surface is smooth, the specific surface energy is large, and other electrochemical active substances loaded on the carbon cloth have poor uniformity and are easy to fall off are solved; in addition, the polyacrylic acid has good shape retention and good mechanical property in the electrolyte; meanwhile, the carbon cloth subjected to polyacrylic acid impregnation treatment is rich in oxygen-containing functional groups and does not need activation treatment, antimony pentoxide grows into a unique mesh porous structure and is uniformly distributed on the surface of the fiber of the flexible carbon cloth, and the flexible electrode combines the flexibility of the carbon cloth and the high specific capacity of the antimony pentoxide, so that the electrochemical cycle performance of the carbon cloth as the cathode material of the sodium-ion battery is integrally improved; the preparation method is simple and novel, and the preparation period is shortAnd the repeatability is high, and the method is suitable for large-scale production and preparation.
Drawings
FIG. 1 is an X-ray diffraction pattern of the negative electrode material of the flexible sodium ion battery with a reticular porous structure of antimony pentoxide/polyacrylic acid/carbon cloth prepared in example 3;
FIG. 2 is a scanning electron micrograph of the negative electrode material of the reticular porous structure antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery prepared in example 3;
fig. 3 is a diagram of the electrochemical cycle performance of the negative electrode material of the flexible sodium ion battery with the reticular porous structure antimony pentoxide/polyacrylic acid/carbon cloth prepared in example 3.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: placing a 4 cm-2 cm hydrophilic carbon cloth into 50mL acetone, soaking for 24h to remove surface impurities, respectively and repeatedly cleaning with deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to dry at 60 ℃; placing the dried carbon cloth into 1mg/mL polyacrylic acid aqueous solution, keeping the carbon cloth for 1h for coating treatment, respectively and repeatedly cleaning the carbon cloth by using deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to be dried again at 60 ℃; wherein, polyacrylic acid has an average molecular weight of 1250000;
step 2: adding 0.3g of antimony trichloride into 20mL of absolute ethyl alcohol, magnetically stirring to form an antimony trichloride solution, adding 0.06g/mL of sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value of the aqueous solution to 8 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution and magnetically stirring for 30 min;
and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a polytetrafluoroethylene kettle, placing the polytetrafluoroethylene kettle and the mixed solution in a homogeneous phase reactor, performing hydrothermal reaction for 48 hours at 120 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode material with the mesh porous structure.
Example 2:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: placing a 4 cm-2 cm hydrophilic carbon cloth into 50mL acetone, soaking for 36h to remove surface impurities, respectively and repeatedly cleaning with deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to dry at 60 ℃; placing the dried carbon cloth into 3mg/mL polyacrylic acid aqueous solution, keeping the carbon cloth for 1h for coating treatment, repeatedly cleaning the carbon cloth by using deionized water and absolute ethyl alcohol respectively, and placing the carbon cloth in an oven to be dried again at 60 ℃; wherein, polyacrylic acid has an average molecular weight of 1250000;
step 2: adding 0.57g of antimony trichloride into 20mL of absolute ethyl alcohol, magnetically stirring to form an antimony trichloride solution, adding 0.08g/mL of sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value of the aqueous solution to 10 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution and magnetically stirring for 30 min;
and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a polytetrafluoroethylene kettle, placing the polytetrafluoroethylene kettle and the mixed solution in a homogeneous phase reactor, performing hydrothermal reaction for 48 hours at the temperature of 150 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with the mesh porous structure.
Example 3:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: placing a 4 cm-2 cm hydrophilic carbon cloth into 50mL acetone, soaking for 72h to remove surface impurities, respectively and repeatedly cleaning with deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to dry at 60 ℃; placing the dried carbon cloth into 6mg/mL polyacrylic acid aqueous solution for 3h for coating treatment, repeatedly cleaning the carbon cloth with deionized water and absolute ethyl alcohol respectively, and placing the carbon cloth in an oven for drying at 60 ℃; wherein, polyacrylic acid has an average molecular weight of 1250000;
step 2: adding 0.57g of antimony trichloride into 20mL of absolute ethyl alcohol, magnetically stirring to form an antimony trichloride solution, adding 0.06g/mL of sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value to 9 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution and magnetically stirring for 30 min;
and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a polytetrafluoroethylene kettle, placing the polytetrafluoroethylene kettle and the mixed solution in a homogeneous phase reactor, performing hydrothermal reaction for 12 hours at 180 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode material with the mesh porous structure.
As shown in FIG. 1, the negative electrode material of the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery is analyzed by a Japanese science D/max2000 PCX-ray diffractometer, and the sample and Sb with the PDF number of 11-0690 are found2O5The structures are consistent. When the sample was observed by a field emission scanning electron microscope (FEI S-4800, USA), as shown in FIG. 2, the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a net-shaped porous structure was observed. As shown in figure 3, the prepared antimony pentoxide/polyacrylic acid/carbon cloth is used as a sodium ion battery cathode material to assemble a CR2032 type battery, and a blue light test system is used for carrying out a cycle performance test, so that the battery has high electrochemical capacity and stability.
Example 4:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: placing a 4 cm-2 cm hydrophilic carbon cloth into 50mL acetone, soaking for 72h to remove surface impurities, respectively and repeatedly cleaning with deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to dry at 60 ℃; placing the dried carbon cloth into 8mg/mL polyacrylic acid aqueous solution, keeping the carbon cloth for 1h for coating treatment, repeatedly cleaning the carbon cloth by using deionized water and absolute ethyl alcohol respectively, and placing the carbon cloth in an oven to be dried again at the temperature of 60 ℃; wherein, polyacrylic acid has an average molecular weight of 1250000;
step 2: adding 1.14g of antimony trichloride into 40mL of absolute ethanol, magnetically stirring to form an antimony trichloride solution, adding 0.06g/mL of sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value to 9 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution and magnetically stirring for 30 min;
and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a polytetrafluoroethylene kettle, placing the polytetrafluoroethylene kettle and the mixed solution in a homogeneous phase reactor, performing hydrothermal reaction for 24 hours at 180 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode material with the mesh porous structure.
Example 5:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: placing a 4 cm-2 cm hydrophilic carbon cloth into 50mL acetone, soaking for 72h to remove surface impurities, respectively and repeatedly cleaning with deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to dry at 60 ℃; placing the dried carbon cloth into 6mg/mL polyacrylic acid aqueous solution, keeping the carbon cloth for 2 hours for coating treatment, repeatedly cleaning the carbon cloth by using deionized water and absolute ethyl alcohol respectively, and placing the carbon cloth in an oven to be dried again at 60 ℃; wherein, polyacrylic acid has an average molecular weight of 1250000;
step 2: adding 0.57g of antimony trichloride into 40mL of absolute ethyl alcohol, magnetically stirring to form an antimony trichloride solution, adding 0.06g/mL of sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value of the aqueous solution to 12 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution and magnetically stirring for 30 min;
and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a polytetrafluoroethylene kettle, placing the polytetrafluoroethylene kettle and the mixed solution in a homogeneous phase reactor, performing hydrothermal reaction for 48 hours at 180 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode material with the mesh porous structure.
Example 6:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: placing a 4 cm-2 cm hydrophilic carbon cloth into 50mL acetone, soaking for 48h to remove surface impurities, respectively and repeatedly cleaning with deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to dry at 60 ℃; then placing the dried carbon cloth into 5mg/mL polyacrylic acid aqueous solution for keeping for 12h for coating treatment, repeatedly cleaning the carbon cloth with deionized water and absolute ethyl alcohol respectively, and placing the carbon cloth in an oven for drying at 60 ℃; wherein, polyacrylic acid has an average molecular weight of 1250000;
step 2: adding 1.14g of antimony trichloride into 60mL of absolute ethyl alcohol, magnetically stirring to form an antimony trichloride solution, adding 0.03g/mL of sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value of the aqueous solution to 10 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution and magnetically stirring for 20 min;
and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous phase reactor, performing hydrothermal reaction for 4 hours at 180 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode material with the mesh porous structure.
Example 7:
a preparation method of a antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with a mesh-shaped porous structure comprises the following steps:
step 1: placing a 4 cm-2 cm hydrophilic carbon cloth into 50mL acetone, soaking for 48h to remove surface impurities, respectively and repeatedly cleaning with deionized water and absolute ethyl alcohol, and placing the carbon cloth in an oven to dry at 60 ℃; placing the dried carbon cloth into a 7mg/mL polyacrylic acid aqueous solution for keeping for 1h for coating treatment, repeatedly cleaning the carbon cloth with deionized water and absolute ethyl alcohol respectively, and placing the carbon cloth in an oven for drying at 60 ℃; wherein, polyacrylic acid has an average molecular weight of 1250000;
step 2: adding 0.57g of antimony trichloride into 30mL of absolute ethyl alcohol, magnetically stirring to form an antimony trichloride solution, adding 0.12g/mL of sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value of the aqueous solution to 11 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution and magnetically stirring for 40 min;
and step 3: transferring the carbon cloth and the mixed solution obtained in the step 2 to a polytetrafluoroethylene kettle, placing the polytetrafluoroethylene kettle and the mixed solution in a homogeneous phase reactor, performing hydrothermal reaction for 36 hours at the temperature of 150 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode material with the mesh porous structure.
In conclusion, the carbon cloth is coated by dipping the cleaned carbon cloth in the polyacrylic acid aqueous solution; then taking out the carbon cloth, repeatedly washing the carbon cloth by using deionized water and ethanol, and drying the carbon cloth for later use; and then the dried carbon cloth is put into an antimony trichloride ethanol solution, and a sodium hydroxide aqueous solution is taken as a precipitator to carry out hydrothermal reaction, so as to prepare the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery cathode with a reticular porous structure. The method has the advantages of simple operation and good repeatability, the carbon cloth after the polyacrylic acid impregnation treatment contains rich oxygen-containing functional groups without activation treatment, the antimony pentoxide grows into a unique reticular porous structure and is uniformly distributed on the surface of the fiber of the flexible carbon cloth, and the flexible electrode combines the flexibility of the carbon cloth and the high specific capacity of the antimony pentoxide, thereby integrally improving the electrochemical cycle performance of the cathode material of the sodium-ion battery.
The foregoing is a more detailed description of the present application in connection with specific embodiments thereof, and it is not intended that the present application be limited to the specific embodiments thereof. For those skilled in the art to which the present application pertains, several simple deductions and substitutions can be made without departing from the concept of the present application, and all should be considered as belonging to the protection scope of the present application.

Claims (9)

1. A preparation method of a mesh porous structure antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material is characterized by comprising the following steps:
step 1: soaking the carbon cloth in acetone to remove surface impurities, cleaning and drying, soaking the dried carbon cloth in polyacrylic acid aqueous solution for coating treatment, cleaning and drying;
step 2: adding 0.3-1.14 g of antimony trichloride into 20-60 mL of absolute ethanol, stirring to form an antimony trichloride solution, adding a sodium hydroxide aqueous solution into the antimony trichloride solution, and adjusting the pH value of the aqueous solution to 8-12 to obtain a mixed solution; soaking the coated carbon cloth in the mixed solution;
and step 3: and (3) transferring the carbon cloth and the mixed solution obtained in the step (2) to a reaction kettle for hydrothermal reaction at 120-180 ℃, cooling to room temperature, taking out the carbon cloth, cleaning and drying to obtain the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-shaped porous structure.
2. The preparation method of the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-like porous structure according to claim 1, wherein the carbon cloth in the step 1 is soaked in acetone for 24-72 h.
3. The preparation method of the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery negative electrode material with the mesh-shaped porous structure according to claim 1, wherein the mass concentration of the polyacrylic acid aqueous solution in the step 1 is 1-8 mg/mL, and the time for immersing the dried carbon cloth in the polyacrylic acid aqueous solution for coating treatment is 1-12 h.
4. The method for preparing the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery negative electrode material with the reticular porous structure according to claim 3, wherein the polyacrylic acid has an average molecular weight of 1250000.
5. The method for preparing the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-like porous structure according to claim 1, wherein the cleaning in the step 1 and the step 3 is repeated by using deionized water and ethanol respectively.
6. The method for preparing the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-shaped porous structure according to claim 1, wherein the carbon cloth coated in the step 2 is soaked in the mixed solution and stirred for 20-40 min.
7. The preparation method of the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-like porous structure according to claim 1, wherein the mass concentration of the sodium hydroxide aqueous solution in the step 2 is 0.03-0.12 g/mL.
8. The preparation method of the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-like porous structure according to claim 1, wherein the reaction kettle in the step 3 is a polytetrafluoroethylene kettle, and the carbon cloth and the mixed solution are transferred to the polytetrafluoroethylene kettle and placed in a homogeneous phase reactor for hydrothermal reaction for 4-48 h.
9. The method for preparing the antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium ion battery negative electrode material with the mesh-shaped porous structure according to claim 1, wherein the carbon cloth is hydrophilic carbon cloth and has a specification of 4cm x 2cm.
CN201910548720.4A 2019-06-24 2019-06-24 Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure Active CN110265644B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910548720.4A CN110265644B (en) 2019-06-24 2019-06-24 Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910548720.4A CN110265644B (en) 2019-06-24 2019-06-24 Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure

Publications (2)

Publication Number Publication Date
CN110265644A CN110265644A (en) 2019-09-20
CN110265644B true CN110265644B (en) 2020-10-16

Family

ID=67920767

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910548720.4A Active CN110265644B (en) 2019-06-24 2019-06-24 Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure

Country Status (1)

Country Link
CN (1) CN110265644B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112038607B (en) * 2020-09-09 2021-08-27 陕西科技大学 Carbon cloth loaded flower-shaped Sb2O4@ polyhedral Sb2O5Composite self-supporting electrode material and preparation method thereof
CN112234204A (en) * 2020-10-16 2021-01-15 陕西科技大学 Carbon cloth loaded SiO2Coated Sb2O5Composite self-supporting electrode material and preparation method thereof

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5206096A (en) * 1990-12-31 1993-04-27 Electric Fuel Limited Slurry for use in rechargeable metal-air batteries
CN101714655A (en) * 2009-11-20 2010-05-26 东莞新能源电子科技有限公司 Lithium-ion secondary battery
CN103840125B (en) * 2012-11-23 2015-11-18 中国科学院大连化学物理研究所 A kind of lithium-sulphur cell positive electrode structure and preparation method thereof
CN104617328B (en) * 2014-07-10 2017-05-31 天津东皋膜技术有限公司 A kind of long-life lithium rechargeable battery and its manufacture method
WO2017191650A1 (en) * 2016-05-03 2017-11-09 Msn Laboratories Private Limited Process for the preparation of 5-[[[(2s)-2-amino-3-[4-(aminocarbonyl)-2,6-dimethylphenyl]-1-oxopropyl][(1s)-1-(4-phenyl-1h-imidazol-2-yl)ethyl]amino]methyl-2-methoxybenzoic acid and its polymorphs thereof
CN106784663A (en) * 2016-12-06 2017-05-31 陕西科技大学 A kind of preparation method of the compound carbon cloth anode material of lithium-ion battery of antimony oxide

Also Published As

Publication number Publication date
CN110265644A (en) 2019-09-20

Similar Documents

Publication Publication Date Title
CN107799757B (en) MoS2Nitrogen-doped carbon tube composite material and preparation method and application thereof
CN111199835B (en) Preparation method of nickel cobalt selenium/nickel cobalt double hydroxide composite electrode material with hierarchical structure
CN109192949A (en) Suede shell hollow polyhedral Co is obtained by ZIF-67 multi-panel derivatization9S8@MoS2Method
CN112436118A (en) VO2(B) Carbon cloth self-supporting material and preparation method and application thereof
CN112701268B (en) Flexible integrated carbon-coated tungsten oxide/carbon nanotube film composite electrode and preparation method thereof
CN109559902B (en) Metal organic framework derived cobalt-nickel-boron sulfide material and preparation method and application thereof
CN110265644B (en) Preparation method of antimony pentoxide/polyacrylic acid/carbon cloth flexible sodium-ion battery cathode material with mesh-shaped porous structure
CN111430672B (en) Preparation method and application of silicon dioxide/carbon cloth self-supporting electrode material
CN108242544B (en) Biomass activated carbon-based carbon material, preparation method thereof and application thereof in sodium-ion battery
CN110790248B (en) Iron-doped cobalt phosphide microsphere electrode material with flower-shaped structure and preparation method and application thereof
CN109755552B (en) Carbon-encapsulated titanium oxynitride nanoparticle composite material and preparation method and application thereof
CN103400980A (en) Iron sesquioxide/nickel oxide core-shell nanorod array film as well as preparation method and application thereof
CN113809286B (en) Metal Organic Framework (MOF) catalyzed growth carbon nanotube coated nickel-tin alloy electrode material and preparation method and application thereof
CN111864190B (en) Preparation method of flexible sulfur positive electrode of lithium-sulfur battery
CN110783542A (en) Paper towel derived carbon fiber loaded MoS 2Preparation method of micro-flower composite material and application of micro-flower composite material in lithium-sulfur battery
CN115863666A (en) Preparation method of graphite felt modified electrode for all-vanadium redox flow battery
CN114220971A (en) Three-dimensional ordered cobalt-nitrogen microporous carbon material with strong catalytic action and preparation method and application thereof
CN115249797A (en) Arrayed molybdenum-doped cobalt diselenide composite material and preparation method and application thereof
CN115207285A (en) Molybdenum disulfide @ tungsten disulfide @ carbon cloth electrode material, and preparation method and application thereof
CN114195198A (en) Co2SnO4/C/S composite material and titanium dioxide induced growth method and application thereof
CN114229825A (en) Metal monoatomic-doped three-dimensional porous carbon material and preparation method and application thereof
CN112885613A (en) Nano material and preparation method and application thereof
CN112635201A (en) Flexible all-solid-state asymmetric supercapacitor electrode and preparation method thereof by dividing flexible all-solid-state asymmetric supercapacitor electrode into two parts
CN116621156B (en) Nitrogen-doped porous carbon material and preparation method and application thereof
CN115304036B (en) Preparation method of nickel cobalt selenide-based nano array electrode material with high cycling stability

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant